反应详情

温度

165 °C

A 500-mL high-pressure bomb reactor was charged with 106b (539 mg, 3.57 mmol), ethanol (30 mL) and excess N,N-ethylmethylamine (50 mL). The mixture was heated at 165° C. for 36 h. After this time, the mixture was concentrated and the resulting residue was purified by flash column chromatography (silica, 98:2 ethyl acetate/triethyl-amine) to afford 106c in 59% yield (397 mg) as a yellow solid: mp 127-129° C.; 1H NMR (500 MHz, DMSO-d6) δ 7.93 (s, 1H), 7.42 (dd, J=7.0, 2.5 Hz, 1H), 6.77-6.75 (m, 2H), 4.23 (s, 2H), 3.46 (q, J=7.0 Hz, 2H), 2.94 (s, 3H), 1.06 (t, J=7.0 Hz, 3H); MS (ESI+) m/z 191.1 (M+H).

1. concentrationAfter this time, the mixture was concentrated
2. customthe resulting residue was purified by flash column chromatography (silica, 98:2 ethyl acetate/triethyl-amine)